HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Fluorobenzoyl chloride → HCID 58486919, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Fluorobenzoyl chloride | HCID 9808 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Sodium bicarbonate methylene chloride | HCID 23716255 | — |
| Reactant | 5-(6-Chloro-2,3-dihydro-5-benzofuranyl)-2-pyridinamine | HCID 58486702 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 58486919 | HCID 58486919 | 45.8% |
Reaction Steps
To a solution of 5-(6-chloro-2,3-dihydrobenzo[3,4-b]furan-5-yl)-2-pyridylamine (144) (19 mg, 0.045 mmol) in 1 ml DCM was added 2-fluorobenzoyl chloride (16 μl, 3 eq) followed by addition of DIEA (39 μl). The resulting solution was stirred at r.t. for overnight. The reaction mixture was worked up with aq. NaHCO3/DCM. DCM phase was washed with brine, concentrated to dryness. The residue was dissolved in 1 ml THF/MeOH/H2O (5:4:1) and stirred with 1N NaOH (100 μl) at r.t. for 2 h and before worked up with EA/aq. NaHCO3. Prep HPLC purification furnished N-[5-(6-chloro(2,3-dihydrobenzo[3,4-b]furan-5-yl))(2-pyridyl)](2-fluorophenyl)carboxamide (146) (7.6 mg, yield: 45.8%, purity>95%) as white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08980629B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-df19193bad254176a93c5b66869bb7ad |
| Source note | uspto-grants-2015_03 |